US4374110A - Purification of silicon source materials - Google Patents
Purification of silicon source materials Download PDFInfo
- Publication number
- US4374110A US4374110A US06/273,519 US27351981A US4374110A US 4374110 A US4374110 A US 4374110A US 27351981 A US27351981 A US 27351981A US 4374110 A US4374110 A US 4374110A
- Authority
- US
- United States
- Prior art keywords
- trichlorosilane
- purification
- silicon
- boron
- hsicl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
- C01B33/10794—Purification by forming addition compounds or complexes, the reactant being possibly contained in an adsorbent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Definitions
- This invention relates in general to a process for purifying silicon source materials and more specifically to a process for removing impurities from trichlorosilane or from mixtures of trichlorosilane and silicon tetrachloride.
- polycrystalline silicon are produced by the hydrogen reduction of a silicon bearing reactant gas.
- a silicon bearing reactant gas for example, in a commonly used process trichlorosilane or mixtures of trichlorosilane with other silicon bearing reactants such as silicon tetrachloride are reduced to deposit polycrystalline silicon on a heated filament.
- silicon source gas it is required that the polycrystalline silicon be of extremely high purity. This in turn requires that the silicon source gas be of high purity and be free from trace impurities.
- BCl 3 present as an impurity in HSiCl 3 is complexed by a hydrolysis process in which water vapor is passed over the surface of the trichlorosilane.
- the purified HSiCl 3 is then separated from the partially hydrolyzed polysiloxane residue by distillation.
- this type of purification is carried out in an operating system, however, the system can be quickly clogged up by the copious amounts of solid polysiloxane residue which are formed.
- elemental boron (or phosphorous) can be removed from HSiCl 3 by the addition of iodine or bromine to the HSiCl 3 .
- the boron (or phosphosous) reacts with the iodine or bromine to form iodides or bromides which are readily separated from HSiCl 3 by distillation.
- This purification technique is not effective unless the boron (or phosphorous) is in the elemental state. Thus in most applications this technique is ineffective for the removal of boron and phosphorous compounds.
- trichlorosilane is purified by reacting trichlorosilane with small quantities of oxygen.
- the complex formed by this oxidation reaction in turn reacts with BCl 3 or PCl 3 to form a boron or phosphorous complex which can be removed from the purified trichlorosilane by distillation.
- Preferably about 0.01 to 0.2 mole percent of oxygen is used in the reaction and the reaction is carried out at a temperature between about 170° and 300° C.
- FIG. 1 illustrates the flow and recycling of reactants in a polycrystalline deposition cycle
- FIG. 2 is a flow diagram illustrating apparatus for purification in accordance with the invention.
- the conventional polycrystalline silicon deposition process is illustrated in FIG. 1.
- trichlorosilane 10 and hydrogen 12 are injected into a reactor bell jar 14. Within the bell jar are heated filaments 16.
- the hydrogen and trichlorosilane react at the surface of the filaments to deposit polycrystalline silicon.
- By-products and unreacted trichlorosilane and hydrogen are exhausted from the bell jar at 18.
- the effluent includes, besides hydrogen and trichlorosilane, hydrogen chloride, silicon tetrachloride, other silicon bearing compounds, and those portions of the impurities which were originally contained in the trichlorosilane and which were not incorporated in the deposited polycrystalline silicon.
- the effluent is processed at 20 to separate out hydrogen 22, silicon bearing reactants 23, and hydrogen chloride 24.
- the hydrogen and silicon bearing reactants are recycled as inputs to the silicon deposition process.
- Makeup amounts of trichlorosilane are added to the silicon bearing effluent.
- Trace amounts of boron and phosphorous are typically present in the incoming trichlorosilane. A portion of these impurities is deposited with the polycrystalline silicon as a dopant. The remaining impurities enter the recycling loop and are subsequently returned to the reactor unless removed in some purification step. The amount of impurities in the recycle loop builds up as the process continues. Although the amount of impurities present in the incoming trichlorosilane may be low enough to not have an adverse doping effect of the deposited polycrystalline silicon the amount of impurities resulting from the build up can have such a deleterious effect.
- an improved purification step specifically for removing boron and phosphorous from either trichlorosilane or other silicon bearing reactants including mixtures of trichlorosilane and silicon tetrachloride is provided.
- boron or phosphorous impurities are complexed by heating the silicon bearing compound and adding a metered amount of oxygen.
- a silicon source material 30 enters the purification system and, for convenience and uniformity, flows into a ballast tank 32.
- the silicon source material is in a gaseous or liquid state and may be, for example, a saturated hydrogen-trichlorosilane gas mixture or the halosilane product stream from a polycrystalline silicon reactor apparatus.
- the latter is comprised mainly of trichlorosilane and silicon tetrachloride.
- From the ballast tank the silicon bearing gas passes through a pump 34 and particulate filters 36 to a gas/gas heat exchanger 38 in which the gas stream is initially warmed. After prewarming in the heat exchanger the gas passes through a primary heater 40 where it reaches the desired reaction temperature.
- a carefully controlled amount of oxygen is added at 42. Adding the oxygen to the heated stream of silicon bearing gas results in a chemical reaction (to be described below) which results in the complexing of boron and phosphorous impurites in the gas stream.
- the heated gas stream then passes again through the heat exchanger where the heat is imparted to the incoming gas stream.
- the now cooled gas stream is optionally collected in a holding tank 44, and then continues on to a conventional distillation apparatus 46 where the boron and phosphorous complexes are separated from the silicon gas stream.
- the purified silicon gas stream is then in condition for injection back into the polycrystalline silicon deposition apparatus.
- GCMS gas chromatography mass spectroscopy
- the initial step in this process is the formation of a Cl 3 Si--OH intermediate.
- the evidence for this type of species is that the final boron reaction product is in the form of B--O--Si species which would originate from a B--Cl species reacting with Si--OH.
- the driving force in this reaction is the thermodynamically favorable formation of the strong B--O and H--Cl bonds.
- the initial oxidation of the HSiCl 3 and the competing side reaction represent trichorosilane which is sacrificed in the purification process. To optimize the process it is desirable that this loss of trichorosilane be minimized.
- 1.0 moles of O 2 reacts to complex about 0.38 moles of boron under the conditions specified above.
- the amount of oxygen necessary to purify the silicon source material can thus be adjusted depending on known impurity levels. In general about 0.01 to 0.2 mole percent of oxygen will be adequate to remove boron and phosphorous compounds from the source material without resulting in too severe a loss of the source material itself.
- the quantity of HSiCl 3 consumed during the purification process is reduced further by diluting the HSiCl 3 to be purified with high purity SiCl 4 .
- the initial oxidative purification step is identical with or without SiCl 4 , namely
- both the HSiCl 3 and SiCl 4 are found to be greatly reduced in boron and phosphorous contamination.
- Nitrogen at a flow rate of about 0.2 liters per minute is bubbled through a tank filled with about 3000-3500 grams of HSiCl 3 .
- the nitrogen gas bubbles through the HSiCl 3 the nitrogen becomes saturated and forms a HSiCl 3 /N 2 vapor combination.
- this vapor is then intentionally contaminated with known quantities of BCl 3 .
- High concentrations (about 1.0% in HSiCl 3 ) of BCl 3 are used to facilitate analysis of the purification data.
- the contamination with BCl 3 is accomplished by bubbling nitrogen gas through a tank containing about 500 milliliter BCl 3 to form a saturated BCl 3 /N 2 vapor combination which is then mixed with HSiCl 3 /N 2 vapor at a selected rate.
- flow rates and pressures are adjusted to deliver 3.6 ⁇ 10 -2 moles/min. of HSiCl 3 and 3.6 ⁇ 10 -4 moles/min. of BCl 3 in the gas stream.
- the gas stream is passed through a furnace tube heated to about 180° C. with a residence time of about 20 seconds in the heated tube.
- the effluent stream is sampled approximately every 15 minutes with GCMS equipped for on-line manual injection.
- Oxygen is added at a flow rate of 2.0 ⁇ 10 -4 moles/min.; the resulting BCl 3 in the effluent stream is measured to be reduced to 2.8 ⁇ 10 -4 moles/min.
- the oxygen flow rate is increased to 4 ⁇ 10 -4 moles/min. and the BCl 3 in the effluent drops further to 2.1 ⁇ 10 -4 moles/min.
- the oxidative purification is repeated at temperatures of 200°, 220°, 250°, 300°, 350°, 400°, 450° and 500° C. Reproducible results are obtained for temperatures less than or equal to 300° C. Preferably the process is carried out at about 200° C. Above 300° C. polysiloxane residue is found to build up in the GCMS transfer lines. Also, slightly less complexing of the BCl 3 is found to occur at temperatures over about 300° C.
- the apparatus as depicted in FIG. 2 is used to purify the effluent from a polycrystalline silicon reactor.
- the silicon bearing materials comprise about 25 percent trichlorosilane and balance silicon tetrachloride.
- the boron contaminant level in the mixture of trichlorosilane and silicon tetrachloride is measured to be greater than or equal to about 0.75 ppb (parts per billion).
- the phosphorous contaminant level in the mixture is measured to be greater than or equal to about 0.65 ppb.
- the effluent gas is heated to a temperature of about 180° to 220° C.
- Oxygen at a level of about 0.01 to 0.2 mole O 2 per mole HSiCl 3 is mixed with the silicon bearing vapor.
- the silicon bearing reactants are distilled to remove higher boiling materials.
- the remaining silicon bearing mixture is analyzed and determined to contain less than 0.10 ppb boron and less than 0.18 ppb phosphorous.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US06/273,519 US4374110A (en) | 1981-06-15 | 1981-06-15 | Purification of silicon source materials |
JP57501831A JPS58500895A (ja) | 1981-06-15 | 1982-05-10 | シリコン原材料の精製法 |
DE823248813T DE3248813T1 (de) | 1981-06-15 | 1982-05-10 | Reinigung von siliciumquellenmaterialien |
PCT/US1982/000614 WO1982004434A1 (en) | 1981-06-15 | 1982-05-10 | Purification of silicon source materials |
IT48535/82A IT1148182B (it) | 1981-06-15 | 1982-05-28 | Procedimento per la purificazione di materiali a base di silicio in particolare triclorosilano e suoi miscugli con tetracloruro di silicio, per la produzione di dispositivi a semiconduttore |
US06/409,391 US4409195A (en) | 1981-06-15 | 1982-08-19 | Purification of silicon source materials |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US06/273,519 US4374110A (en) | 1981-06-15 | 1981-06-15 | Purification of silicon source materials |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US06/409,391 Continuation-In-Part US4409195A (en) | 1981-06-15 | 1982-08-19 | Purification of silicon source materials |
Publications (1)
Publication Number | Publication Date |
---|---|
US4374110A true US4374110A (en) | 1983-02-15 |
Family
ID=23044269
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US06/273,519 Expired - Fee Related US4374110A (en) | 1981-06-15 | 1981-06-15 | Purification of silicon source materials |
US06/409,391 Expired - Fee Related US4409195A (en) | 1981-06-15 | 1982-08-19 | Purification of silicon source materials |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US06/409,391 Expired - Fee Related US4409195A (en) | 1981-06-15 | 1982-08-19 | Purification of silicon source materials |
Country Status (5)
Country | Link |
---|---|
US (2) | US4374110A (ja) |
JP (1) | JPS58500895A (ja) |
DE (1) | DE3248813T1 (ja) |
IT (1) | IT1148182B (ja) |
WO (1) | WO1982004434A1 (ja) |
Cited By (22)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4585643A (en) * | 1985-05-31 | 1986-04-29 | Union Carbide Corporation | Process for preparing chlorosilanes from silicon and hydrogen chloride using an oxygen promoter |
US4892568A (en) * | 1988-02-19 | 1990-01-09 | Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe Mbh | Process for removing n-type impurities from liquid or gaseous substances produced in the gas-phase deposition of silicon |
US5232602A (en) * | 1992-07-01 | 1993-08-03 | Hemlock Semiconductor Corporation | Phosphorous removal from tetrachlorosilane |
US20040039219A1 (en) * | 2001-12-13 | 2004-02-26 | Tianniu Chen | Stabilized cyclosiloxanes for use as CVD precursors for low-dielectric constant thin films |
US7108771B2 (en) | 2001-12-13 | 2006-09-19 | Advanced Technology Materials, Inc. | Method for removal of impurities in cyclic siloxanes useful as precursors for low dielectric constant thin films |
CN100345753C (zh) * | 2006-03-10 | 2007-10-31 | 锦州铁合金股份有限公司 | 锆英砂沸腾氯化反应中产生的四氯化硅的回收提纯方法 |
US7342295B2 (en) | 2002-11-21 | 2008-03-11 | Advanced Technology Materials, Inc. | Porogen material |
US20090016947A1 (en) * | 2006-03-03 | 2009-01-15 | Wacker Chemie Ag | Recycling of high-boiling compounds within an integrated chlorosilane system |
US20090068081A1 (en) * | 2007-09-05 | 2009-03-12 | Shin -Etsu Chemical Co., Ltd. | Method for purifying chlorosilanes |
US20100124525A1 (en) * | 2008-11-19 | 2010-05-20 | Kuyen Li | ZERO-HEAT-BURDEN FLUIDIZED BED REACTOR FOR HYDRO-CHLORINATION OF SiCl4 and M.G.-Si |
US20110052474A1 (en) * | 2008-01-14 | 2011-03-03 | Evonik Degussa Gmbh | Installation and method for reducing the content in elements, such as boron, of halosilanes |
US20110129621A1 (en) * | 2008-03-26 | 2011-06-02 | Gt Solar, Incorporated | Systems and methods for distributing gas in a chemical vapor deposition reactor |
US8053375B1 (en) | 2006-11-03 | 2011-11-08 | Advanced Technology Materials, Inc. | Super-dry reagent compositions for formation of ultra low k films |
EP2385017A1 (en) | 2010-05-05 | 2011-11-09 | Shyang Su | Process for purifying silicon source material by high gravity roating packed beds |
CN102241402A (zh) * | 2010-05-14 | 2011-11-16 | 苏翔 | 以超重力旋转填充床纯化硅原料的制造方法 |
WO2012099700A1 (en) * | 2010-12-31 | 2012-07-26 | Solexel, Inc. | Deposition systems and processes |
CN102666381A (zh) * | 2009-12-04 | 2012-09-12 | 斯帕恩特私人有限公司 | 制备卤化聚硅烷的方法 |
US8568597B2 (en) | 2010-05-10 | 2013-10-29 | Shyang Su | Process for purifying silicon source material by high gravity rotating packed beds |
US9193597B2 (en) | 2009-08-12 | 2015-11-24 | Shin-Etsu Chemical Co., Ltd. | Method for purifying chlorosilanes |
US9870937B2 (en) | 2010-06-09 | 2018-01-16 | Ob Realty, Llc | High productivity deposition reactor comprising a gas flow chamber having a tapered gas flow space |
CN108946743A (zh) * | 2018-09-28 | 2018-12-07 | 洛阳中硅高科技有限公司 | 提纯三氯氢硅的方法 |
CN113302153A (zh) * | 2019-01-22 | 2021-08-24 | 株式会社德山 | 纯化氯硅烷类的制造方法 |
Families Citing this family (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4529707A (en) * | 1982-09-21 | 1985-07-16 | General Electric Company | Detection of boron impurities in chlorosilanes |
US5094830A (en) * | 1987-03-24 | 1992-03-10 | Novapure Corporation | Process for removal of water and silicon mu-oxides from chlorosilanes |
US5503816A (en) * | 1993-09-27 | 1996-04-02 | Becton Dickinson And Company | Silicate compounds for DNA purification |
US5900532A (en) | 1997-02-20 | 1999-05-04 | Nippon Sanso Corporation | Method of removing siloxanes from silicon compound gases and apparatus therefor |
US5723644A (en) * | 1997-04-28 | 1998-03-03 | Dow Corning Corporation | Phosphorous removal from chlorosilane |
DE10048504C2 (de) * | 2000-09-29 | 2002-10-17 | Messer Griesheim Gmbh | Verfahren zur Herstellung von Chlorsilanen mit niedrigem Dotierstoffgehalt |
ITRM20040570A1 (it) | 2004-11-19 | 2005-02-19 | Memc Electronic Materials | Procedimento e impianto di purificazione di triclorosilano e di tetracloruro di silicio. |
JP4714196B2 (ja) | 2007-09-05 | 2011-06-29 | 信越化学工業株式会社 | トリクロロシランの製造方法および多結晶シリコンの製造方法 |
JP4659798B2 (ja) | 2007-09-05 | 2011-03-30 | 信越化学工業株式会社 | トリクロロシランの製造方法 |
JP4714197B2 (ja) | 2007-09-05 | 2011-06-29 | 信越化学工業株式会社 | トリクロロシランの製造方法および多結晶シリコンの製造方法 |
DE102008004397A1 (de) * | 2008-01-14 | 2009-07-16 | Evonik Degussa Gmbh | Verfahren zur Verminderung des Gehaltes von Elementen, wie Bor, in Halogensilanen sowie Anlage zur Durchführung des Verfahrens |
WO2010074674A1 (en) * | 2008-12-23 | 2010-07-01 | Arise Technologies Corporation | Method and apparatus for silicon refinement |
JP5210350B2 (ja) * | 2010-05-17 | 2013-06-12 | 翔 蘇 | 回転充填層によりシリコンを精製する方法 |
CN101913609A (zh) * | 2010-08-19 | 2010-12-15 | 天威四川硅业有限责任公司 | 三氯氢硅混合气除杂处理方法和装置 |
JP5542026B2 (ja) | 2010-10-27 | 2014-07-09 | 信越化学工業株式会社 | クロロシラン類の精製方法 |
JP5507498B2 (ja) * | 2011-06-21 | 2014-05-28 | 信越化学工業株式会社 | クロロシラン類の精製方法 |
US10011493B2 (en) * | 2012-04-27 | 2018-07-03 | Corner Star Limited | Methods for purifying halosilane-containing streams |
JP5909153B2 (ja) | 2012-06-14 | 2016-04-26 | 信越化学工業株式会社 | 高純度多結晶シリコンの製造方法 |
JP6095613B2 (ja) * | 2014-07-10 | 2017-03-15 | 信越化学工業株式会社 | クロロシランの精製方法 |
CN107344146B (zh) * | 2016-05-06 | 2019-10-18 | 芯米(厦门)半导体设备有限公司 | 液态纯化材料的设备 |
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US3540861A (en) * | 1968-02-07 | 1970-11-17 | Union Carbide Corp | Purification of silicon compounds |
US3871872A (en) * | 1973-05-30 | 1975-03-18 | Union Carbide Corp | Method for promoting metallurgical reactions in molten metal |
-
1981
- 1981-06-15 US US06/273,519 patent/US4374110A/en not_active Expired - Fee Related
-
1982
- 1982-05-10 JP JP57501831A patent/JPS58500895A/ja active Granted
- 1982-05-10 WO PCT/US1982/000614 patent/WO1982004434A1/en active Application Filing
- 1982-05-10 DE DE823248813T patent/DE3248813T1/de active Granted
- 1982-05-28 IT IT48535/82A patent/IT1148182B/it active
- 1982-08-19 US US06/409,391 patent/US4409195A/en not_active Expired - Fee Related
Patent Citations (3)
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US3252752A (en) * | 1958-01-11 | 1966-05-24 | Licentia Gmbh | Method for producing pure silane and chlorinated silanes |
US3540861A (en) * | 1968-02-07 | 1970-11-17 | Union Carbide Corp | Purification of silicon compounds |
US3871872A (en) * | 1973-05-30 | 1975-03-18 | Union Carbide Corp | Method for promoting metallurgical reactions in molten metal |
Cited By (34)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4585643A (en) * | 1985-05-31 | 1986-04-29 | Union Carbide Corporation | Process for preparing chlorosilanes from silicon and hydrogen chloride using an oxygen promoter |
US4892568A (en) * | 1988-02-19 | 1990-01-09 | Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe Mbh | Process for removing n-type impurities from liquid or gaseous substances produced in the gas-phase deposition of silicon |
US5232602A (en) * | 1992-07-01 | 1993-08-03 | Hemlock Semiconductor Corporation | Phosphorous removal from tetrachlorosilane |
US7423166B2 (en) | 2001-12-13 | 2008-09-09 | Advanced Technology Materials, Inc. | Stabilized cyclosiloxanes for use as CVD precursors for low-dielectric constant thin films |
US20040039219A1 (en) * | 2001-12-13 | 2004-02-26 | Tianniu Chen | Stabilized cyclosiloxanes for use as CVD precursors for low-dielectric constant thin films |
US7108771B2 (en) | 2001-12-13 | 2006-09-19 | Advanced Technology Materials, Inc. | Method for removal of impurities in cyclic siloxanes useful as precursors for low dielectric constant thin films |
US20060235182A1 (en) * | 2001-12-13 | 2006-10-19 | Chongying Xu | Method for removal of impurities in cyclic siloxanes useful as precursors for low dielectric constant thin films |
US7342295B2 (en) | 2002-11-21 | 2008-03-11 | Advanced Technology Materials, Inc. | Porogen material |
US20090016947A1 (en) * | 2006-03-03 | 2009-01-15 | Wacker Chemie Ag | Recycling of high-boiling compounds within an integrated chlorosilane system |
US8557210B2 (en) | 2006-03-03 | 2013-10-15 | Wacker Chemie Ag | Recycling of high-boiling compounds within an integrated chlorosilane system |
CN100345753C (zh) * | 2006-03-10 | 2007-10-31 | 锦州铁合金股份有限公司 | 锆英砂沸腾氯化反应中产生的四氯化硅的回收提纯方法 |
US8053375B1 (en) | 2006-11-03 | 2011-11-08 | Advanced Technology Materials, Inc. | Super-dry reagent compositions for formation of ultra low k films |
US20090068081A1 (en) * | 2007-09-05 | 2009-03-12 | Shin -Etsu Chemical Co., Ltd. | Method for purifying chlorosilanes |
EP2036858A3 (en) * | 2007-09-05 | 2009-07-22 | Shinetsu Chemical Co., Ltd. | Method for purifying chlorosilanes |
US20110052474A1 (en) * | 2008-01-14 | 2011-03-03 | Evonik Degussa Gmbh | Installation and method for reducing the content in elements, such as boron, of halosilanes |
US8961689B2 (en) * | 2008-03-26 | 2015-02-24 | Gtat Corporation | Systems and methods for distributing gas in a chemical vapor deposition reactor |
US20110129621A1 (en) * | 2008-03-26 | 2011-06-02 | Gt Solar, Incorporated | Systems and methods for distributing gas in a chemical vapor deposition reactor |
US20100124525A1 (en) * | 2008-11-19 | 2010-05-20 | Kuyen Li | ZERO-HEAT-BURDEN FLUIDIZED BED REACTOR FOR HYDRO-CHLORINATION OF SiCl4 and M.G.-Si |
US9193597B2 (en) | 2009-08-12 | 2015-11-24 | Shin-Etsu Chemical Co., Ltd. | Method for purifying chlorosilanes |
US9458294B2 (en) | 2009-12-04 | 2016-10-04 | Spawnt Private S.À.R.L. | Method for removing impurities from silicon |
US9040009B2 (en) | 2009-12-04 | 2015-05-26 | Spawnt Private S.à.r.1. | Kinetically stable chlorinated polysilanes and production thereof |
US9139702B2 (en) | 2009-12-04 | 2015-09-22 | Spawnt Private S.A.R.L. | Method for producing halogenated polysilanes |
CN102666381B (zh) * | 2009-12-04 | 2014-12-31 | 斯帕恩特私人有限公司 | 制备卤化聚硅烷的方法 |
CN102666381A (zh) * | 2009-12-04 | 2012-09-12 | 斯帕恩特私人有限公司 | 制备卤化聚硅烷的方法 |
EP2385017A1 (en) | 2010-05-05 | 2011-11-09 | Shyang Su | Process for purifying silicon source material by high gravity roating packed beds |
US8568597B2 (en) | 2010-05-10 | 2013-10-29 | Shyang Su | Process for purifying silicon source material by high gravity rotating packed beds |
CN102241402A (zh) * | 2010-05-14 | 2011-11-16 | 苏翔 | 以超重力旋转填充床纯化硅原料的制造方法 |
US9870937B2 (en) | 2010-06-09 | 2018-01-16 | Ob Realty, Llc | High productivity deposition reactor comprising a gas flow chamber having a tapered gas flow space |
KR101368598B1 (ko) | 2010-12-31 | 2014-03-05 | 솔렉셀, 인크. | 증착 시스템 및 공정 |
WO2012099700A1 (en) * | 2010-12-31 | 2012-07-26 | Solexel, Inc. | Deposition systems and processes |
CN108946743A (zh) * | 2018-09-28 | 2018-12-07 | 洛阳中硅高科技有限公司 | 提纯三氯氢硅的方法 |
CN113302153A (zh) * | 2019-01-22 | 2021-08-24 | 株式会社德山 | 纯化氯硅烷类的制造方法 |
US20220073358A1 (en) * | 2019-01-22 | 2022-03-10 | Tokuyama Corporation | Method for Producing Refined Chlorosilane |
CN113302153B (zh) * | 2019-01-22 | 2023-12-26 | 株式会社德山 | 纯化氯硅烷类的制造方法 |
Also Published As
Publication number | Publication date |
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IT8248535A0 (it) | 1982-05-28 |
US4409195A (en) | 1983-10-11 |
DE3248813T1 (de) | 1983-06-16 |
JPS641407B2 (ja) | 1989-01-11 |
WO1982004434A1 (en) | 1982-12-23 |
DE3248813C2 (ja) | 1988-09-22 |
IT1148182B (it) | 1986-11-26 |
JPS58500895A (ja) | 1983-06-02 |
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